CN107880763B - Waterproof environment-friendly coating and preparation method thereof - Google Patents
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Abstract
The invention discloses a waterproof environment-friendly coating and a preparation method thereof, and the preparation method of the waterproof environment-friendly coating has the advantages of simple preparation process and low production cost; after the waterproof environment-friendly coating disclosed by the invention is used, the waterproof performance can be effectively improved, the waterproof environment-friendly coating has unique waterproofness, high elasticity and integrity, a coating film is continuous without any seam and is leakage-resistant, the coating film has good cohesiveness to various base materials of a building, is not easy to peel, and has the advantages of excellent anticorrosion effect, good anti-aging effect, strong decoration, good durability and the like. The preparation method comprises the following steps: s1, weighing the raw materials; s2, preparing a solution A; s3, preparing a solution B; s4, adding kaolin and calcium carbonate into the solution B, keeping the pressure of the synthesis kettle between-0.12 MPa and-0.08 MPa, stirring for 2-4 hours at room temperature, and discharging to obtain the catalyst.
Description
Technical Field
The invention relates to a waterproof coating, in particular to a waterproof environment-friendly coating and a preparation method thereof.
Background
Waterproofing has long been no longer a fresh topic, and is not negligible in tunnels, bridges, dams, roads, buildings and houses where people live in daily life. The waterproof film formed by curing the waterproof coating has certain extensibility, elastoplasticity, crack resistance, impermeability and weather resistance, and can play roles in waterproofing, seepage prevention and protection. The waterproof coating has good temperature adaptability, is simple and convenient to operate and is easy to maintain.
Chinese patent (application number: 201110344194.3) discloses a waterproof paint, which consists of the following components: 30-50% of styrene-acrylic emulsion, 25-30% of stone powder, 0-5% of heavy calcium carbonate, 1-5% of an anti-aging agent, 0-5% of a defoaming agent, 0-5% of talcum powder, 3-5% of titanium dioxide, 5-10% of polyvinyl alcohol, 1-5% of sodium hexametaphosphate and 10% of water.
Chinese patent (application No. 201510890818.X) discloses a waterproof coating which comprises, by weight, 10-20 parts of cement, 1-3 parts of calcium carbonate, 5-8 parts of quartz sand, 20-36 parts of acrylic elastic emulsion, 1-5 parts of nano silicon oxide, 8-15 parts of inert inorganic powder, 1-3 parts of a dispersing agent, 1-10 parts of a defoaming agent, 1-5 parts of a flame retardant, 1-5 parts of heavy calcium carbonate, 1-3 parts of a silane coupling agent, 7-18 parts of water, 3-10 parts of an emulsifier and 2-10 parts of polyethylene glycol.
Chinese patent (application No. 201610359498.X) discloses a waterproof coating which is prepared from the following raw materials in parts by weight: 100 parts of polyacrylic resin, 15-20 parts of rosin, 1-5 parts of zinc stearate, 6-10 parts of safflower oil, 6-10 parts of petroleum, 5-8 parts of isobutyl triethoxy silicon, 1-5 parts of potassium hydroxide, 0.1-0.2 part of sodium metabisulfite, 20-30 parts of pigment and 15-20 parts of deionized water with the conductivity of less than 5 mu S/cm.
However, the existing waterproof coating cannot effectively resist rain and scouring for a long time. As a result, it is often seen that decorated and painted, clean and aesthetically pleasing buildings are mottled in color by not withstanding rain and wind erosion and moisture. Mainly, the coatings lack inorganic substances with stable chemical properties and water insolubility, and the performance of the coatings is not similar to the physical performance of a building body. Therefore, the effect of comprehensive waterproof performance is not good.
Disclosure of Invention
The invention provides a waterproof environment-friendly coating and a preparation method thereof, so that the flame retardant and waterproof functions of the coating are realized, and the use safety of the coating is improved.
The technical scheme is as follows:
a preparation method of a waterproof environment-friendly coating comprises the following steps:
s1, weighing the following raw materials: polyester, polyether, a softening agent, kaolin, calcium carbonate, a coupling agent, 3-hydroxyethyl-1, 3-oxazolidine, a catalyst and 1, 6-hexamethylene diisocyanate;
s2, adding polyether and polyester into a reaction kettle, removing vacuum after vacuum dehydration, cooling to 75-85 ℃, adding 1, 6-hexamethylene diisocyanate, stirring for 2-4 hours at the rotating speed, adding a softening agent, and stirring for 20-40 minutes to obtain a solution A;
s3, pumping the solution A into a synthesis kettle, keeping the pressure of the synthesis kettle at-0.12 to-0.08 MPa, sequentially adding 3-hydroxyethyl-1, 3-oxazolidine, a catalyst and a coupling agent at room temperature, and stirring for 5-15 minutes to obtain a solution B;
s4, adding kaolin and calcium carbonate into the solution B, keeping the pressure of the synthesis kettle between-0.12 MPa and-0.08 MPa, stirring for 2-4 hours at room temperature, and discharging to obtain the catalyst.
A preparation method of a waterproof environment-friendly coating comprises the following steps:
s1, weighing the following raw materials in parts by weight: 25-30 parts of polyester, 48-52 parts of polyether, 1.5-4.5 parts of softener, 15-25 parts of kaolin, 5-15 parts of calcium carbonate, 0.3-0.7 part of coupling agent, 0.4-0.9 part of 3-hydroxyethyl-1, 3-oxazolidine, 0.3-0.6 part of catalyst and 15-20 parts of 1, 6-hexamethylene diisocyanate;
s2, adding polyether and polyester into a reaction kettle, raising the temperature to 110 ℃ for 100-;
s3, pumping the solution A into a synthesis kettle, keeping the pressure of the synthesis kettle between-0.12 and-0.08 MPa, and sequentially adding 3-hydroxyethyl-1, 3-oxazolidine, a catalyst and a coupling agent at the room temperature and stirring at 600 revolutions per minute for 5 to 15 minutes to obtain a solution B;
s4, adding kaolin and calcium carbonate into the solution B, keeping the pressure of the synthesis kettle between-0.12 MPa and-0.08 MPa, stirring at the speed of 600 revolutions per minute for 2 to 4 hours at room temperature, and discharging to obtain the catalyst.
The coupling agent is N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane.
The coupling agent is brominated bisphenol A epoxy resin modified N- (2-N-benzyl aminoethyl) -3-aminopropyltrimethoxysilane.
The preparation process of the brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane comprises the following steps: brominated bisphenol A epoxy resin and acetone are mixed according to the mass ratio of 1: (2-4) adding the mixture into a three-neck flask filled with nitrogen, stirring the mixture for 5 to 15 minutes at the rotating speed of 60 to 180 r/min, uniformly mixing the mixture, adding N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane, the weight of which is 1.5 to 2.5 times that of the brominated bisphenol A epoxy resin, into the mixture, and stirring the mixture at the rotating speed of 60 to 180 r/min at room temperature for reacting the mixture for 50 to 80 minutes to obtain a reactant; and (3) distilling the reactant at the temperature of 45-55 ℃ and the vacuum degree of-0.12 to-0.09 MPa under reduced pressure to remove acetone to obtain the brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane.
The catalyst is one or a mixture of cobalt naphthenate, dibutyltin dilaurate and stannous octoate.
The softener is one or a mixture of more of dibutyl phthalate, dioctyl phthalate and neopentyl glycol 2, 2-dimethyl-3-hydroxypropionate. In one embodiment of the present invention, the softener consists of 23 to 35 wt% dioctyl phthalate and 65 to 75 wt% neopentyl glycol 2, 2-dimethyl-3-hydroxypropionate.
The particle size of the kaolin is 1000-1500 meshes.
The calcium carbonate is light calcium carbonate with the particle size of 1000-1500 meshes.
The polyester is unsaturated polyester resin, and the acid value is 10-30 mgKOH/g.
The hydroxyl value of the polyether is 15-45 mgKOH/g.
The epoxy equivalent of the brominated bisphenol A epoxy resin is 300-500g/eq, and the bromine content is 10-30 wt%.
A waterproof environment-friendly coating is prepared by the preparation method.
The technical effects are as follows:
the waterproof environment-friendly coating and the preparation method thereof have the advantages of simple preparation process and low production cost; after the waterproof environment-friendly coating disclosed by the invention is used, the waterproof performance can be effectively improved, the waterproof environment-friendly coating has unique waterproofness, high elasticity and integrity, a coating film is continuous without any seam and is leakage-resistant, the coating film has good cohesiveness to various base materials of a building, is not easy to peel, and has the advantages of excellent anticorrosion effect, good anti-aging effect, strong decoration, good durability and the like.
Detailed Description
In the examples, the kaolin was a 1250 mesh calcined kaolin provided by Shanghai Yangtze titanium white chemical products Co., Ltd., and was in the form of white powder.
The precipitated calcium carbonate in the examples is 1250 mesh active precipitated calcium carbonate available from Suzhou famous craftsman Fine chemical Co., Ltd. under model No. MJ-HXQG.
Examples 1, 6-hexamethylene diisocyanate, CAS number: 822-06-0.
In the examples, the polyester is an unsaturated polyester resin with a model number of 168-2Q provided by Idison chemical Co., Ltd, of Foshan, and the acid value is 18-23 mgKOH/g.
In the embodiment, the polyether is provided by Shandong Lanxingdong chemical industry, Limited liability company and has a grade of DL-3000D, and the hydroxyl value is 36-39 mgKOH/g.
Examples N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane, CAS No.: 209866-89-7.
In the examples, the brominated bisphenol A epoxy resin is provided by Taiwan south Asia plastic industry Co., Ltd under the trade name of NPEB-450A80, the epoxy equivalent is 410-440g/eq, and the bromine content is 18-21 wt%.
Examples acetone, CAS number: 67-64-1.
Cobalt naphthenate, CAS number: 61789-51-3.
Examples dioctyl phthalate, CAS number: 117-84-0.
Example 2, 2-dimethyl-3-hydroxypropionic acid neopentyl glycol ester, CAS number: 1115-20-4.
In the examples, 3-hydroxyethyl-1, 3-oxazolidine is prepared by methods in section 1.2 of "Synthesis and characterization of 3-hydroxyethyl-1, 3-oxazolidine and preliminary application thereof" by Hippocampus et al.
Example 1
The preparation method of the waterproof environment-friendly coating comprises the following steps:
s1, weighing the following raw materials in parts by weight: 28 parts of polyester, 50 parts of polyether, 3 parts of 2, 2-dimethyl-3-hydroxypropionic acid neopentyl glycol ester, 20 parts of kaolin, 10 parts of calcium carbonate, 0.5 part of N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane, 0.6 part of 3-hydroxyethyl-1, 3-oxazolidine, 0.5 part of cobalt naphthenate and 18 parts of 1, 6-hexamethylene diisocyanate;
s2, adding polyether and polyester into a reaction kettle, raising the temperature to 105 ℃, reducing the pressure to-0.095 MPa, dehydrating in vacuum for 30 minutes, removing the vacuum, reducing the temperature to 80 ℃, adding 1, 6-hexamethylene diisocyanate, stirring for 3 hours at the rotating speed of 400 rpm, adding 2, 2-dimethyl-3-neopentyl glycol hydroxypropionate, and stirring for 30 minutes at the rotating speed of 400 rpm to obtain a solution A;
s3, pumping the solution A into a synthesis kettle, keeping the pressure of the synthesis kettle at-0.1 MPa, and sequentially adding 3-hydroxyethyl-1, 3-oxazolidine, cobalt naphthenate and N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane into the synthesis kettle at room temperature of 25 ℃ to stir for 10 minutes at 450 revolutions per minute to obtain a solution B;
s4, adding kaolin and calcium carbonate into the solution B, keeping the pressure of the synthesis kettle at-0.1 MPa, stirring at the room temperature of 25 ℃ for 5 hours at 450 rpm, and discharging to obtain the waterproof environment-friendly coating.
Example 2
The preparation method of the waterproof environment-friendly coating comprises the following steps:
s1, weighing the following raw materials in parts by weight: 28 parts of polyester, 50 parts of polyether, 3 parts of 2, 2-dimethyl-3-hydroxypropionic acid neopentyl glycol ester, 20 parts of kaolin, 10 parts of calcium carbonate, 0.5 part of coupling agent, 0.6 part of 3-hydroxyethyl-1, 3-oxazolidine, 0.5 part of cobalt naphthenate and 18 parts of 1, 6-hexamethylene diisocyanate;
s2, adding polyether and polyester into a reaction kettle, raising the temperature to 105 ℃, reducing the pressure to-0.095 MPa, dehydrating in vacuum for 30 minutes, removing the vacuum, reducing the temperature to 80 ℃, adding 1, 6-hexamethylene diisocyanate, stirring for 3 hours at the rotating speed of 400 rpm, adding 2, 2-dimethyl-3-neopentyl glycol hydroxypropionate, and stirring for 30 minutes at the rotating speed of 400 rpm to obtain a solution A;
s3, pumping the solution A into a synthesis kettle, keeping the pressure of the synthesis kettle at-0.1 MPa, sequentially adding 3-hydroxyethyl-1, 3-oxazolidine, cobalt naphthenate and a coupling agent at room temperature of 25 ℃, and stirring for 10 minutes at 450 revolutions per minute to obtain a solution B;
s4, adding kaolin and calcium carbonate into the solution B, keeping the pressure of the synthesis kettle at-0.1 MPa, stirring at the room temperature of 25 ℃ for 5 hours at 450 rpm, and discharging to obtain the waterproof environment-friendly coating.
The coupling agent is brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane, and the preparation process of the brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane is as follows: brominated bisphenol A epoxy resin and acetone are mixed according to the mass ratio of 1: 3 adding the mixture into a three-neck flask filled with nitrogen, stirring the mixture for 10 minutes at the rotating speed of 120 revolutions per minute, uniformly mixing the mixture, and then adding N- (2-N-benzyl aminoethyl) -3-aminopropyl trimethoxy silane which is 2 times of the weight of brominated bisphenol A epoxy resin, stirring the mixture at the rotating speed of 90 revolutions per minute at room temperature, and reacting the mixture for 60 minutes to obtain a reactant; and (3) distilling the reactant at 50 ℃ and the vacuum degree of-0.1 MPa under reduced pressure to remove acetone to obtain the brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane.
Example 3
The preparation method of the waterproof environment-friendly coating comprises the following steps:
s1, weighing the following raw materials in parts by weight: 28 parts of polyester, 50 parts of polyether, 3 parts of dioctyl phthalate, 20 parts of kaolin, 10 parts of calcium carbonate, 0.5 part of coupling agent, 0.6 part of 3-hydroxyethyl-1, 3-oxazolidine, 0.5 part of cobalt naphthenate and 18 parts of 1, 6-hexamethylene diisocyanate;
s2, adding polyether and polyester into a reaction kettle, raising the temperature to 105 ℃, reducing the pressure to-0.095 MPa, dehydrating in vacuum for 30 minutes, removing the vacuum, reducing the temperature to 80 ℃, adding 1, 6-hexamethylene diisocyanate, stirring for 3 hours at the rotating speed of 400 revolutions per minute, adding dioctyl phthalate, and stirring for 30 minutes at the rotating speed of 400 revolutions per minute to obtain a solution A;
s3, pumping the solution A into a synthesis kettle, keeping the pressure of the synthesis kettle at-0.1 MPa, sequentially adding 3-hydroxyethyl-1, 3-oxazolidine, cobalt naphthenate and a coupling agent at room temperature of 25 ℃, and stirring for 10 minutes at 450 revolutions per minute to obtain a solution B;
s4, adding kaolin and calcium carbonate into the solution B, keeping the pressure of the synthesis kettle at-0.1 MPa, stirring at the room temperature of 25 ℃ for 5 hours at 450 rpm, and discharging to obtain the waterproof environment-friendly coating.
The coupling agent is brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane, and the preparation process of the brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane is as follows: brominated bisphenol A epoxy resin and acetone are mixed according to the mass ratio of 1: 3 adding the mixture into a three-neck flask filled with nitrogen, stirring the mixture for 10 minutes at the rotating speed of 120 revolutions per minute, uniformly mixing the mixture, and then adding N- (2-N-benzyl aminoethyl) -3-aminopropyl trimethoxy silane which is 2 times of the weight of brominated bisphenol A epoxy resin, stirring the mixture at the rotating speed of 90 revolutions per minute at room temperature, and reacting the mixture for 60 minutes to obtain a reactant; and (3) distilling the reactant at 50 ℃ and the vacuum degree of-0.1 MPa under reduced pressure to remove acetone to obtain the brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane.
Example 4
The preparation method of the waterproof environment-friendly coating comprises the following steps:
s1, weighing the following raw materials in parts by weight: 28 parts of polyester, 50 parts of polyether, 3 parts of dibutyl phthalate, 20 parts of kaolin, 10 parts of calcium carbonate, 0.5 part of coupling agent, 0.6 part of 3-hydroxyethyl-1, 3-oxazolidine, 0.5 part of cobalt naphthenate and 18 parts of 1, 6-hexamethylene diisocyanate;
s2, adding polyether and polyester into a reaction kettle, raising the temperature to 105 ℃, reducing the pressure to-0.095 MPa, carrying out vacuum dehydration for 30 minutes, removing vacuum, reducing the temperature to 80 ℃, adding 1, 6-hexamethylene diisocyanate, stirring for 3 hours at the rotating speed of 400 rpm, adding dibutyl phthalate, and stirring for 30 minutes at the rotating speed of 400 rpm to obtain a solution A;
s3, pumping the solution A into a synthesis kettle, keeping the pressure of the synthesis kettle at-0.1 MPa, sequentially adding 3-hydroxyethyl-1, 3-oxazolidine, cobalt naphthenate and a coupling agent at room temperature of 25 ℃, and stirring for 10 minutes at 450 revolutions per minute to obtain a solution B;
s4, adding kaolin and calcium carbonate into the solution B, keeping the pressure of the synthesis kettle at-0.1 MPa, stirring at the room temperature of 25 ℃ for 5 hours at 450 rpm, and discharging to obtain the waterproof environment-friendly coating.
The coupling agent is brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane, and the preparation process of the brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane is as follows: brominated bisphenol A epoxy resin and acetone are mixed according to the mass ratio of 1: 3 adding the mixture into a three-neck flask filled with nitrogen, stirring the mixture for 10 minutes at the rotating speed of 120 revolutions per minute, uniformly mixing the mixture, and then adding N- (2-N-benzyl aminoethyl) -3-aminopropyl trimethoxy silane which is 2 times of the weight of brominated bisphenol A epoxy resin, stirring the mixture at the rotating speed of 90 revolutions per minute at room temperature, and reacting the mixture for 60 minutes to obtain a reactant; and (3) distilling the reactant at 50 ℃ and the vacuum degree of-0.1 MPa under reduced pressure to remove acetone to obtain the brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane.
Example 5
The preparation method of the waterproof environment-friendly coating comprises the following steps:
s1, weighing the following raw materials in parts by weight: 28 parts of polyester, 50 parts of polyether, 2.1 parts of 2, 2-dimethyl-3-hydroxypropionic acid neopentyl glycol ester, 0.9 part of dioctyl phthalate, 20 parts of kaolin, 10 parts of calcium carbonate, 0.5 part of coupling agent, 0.6 part of 3-hydroxyethyl-1, 3-oxazolidine, 0.5 part of cobalt naphthenate and 18 parts of 1, 6-hexamethylene diisocyanate;
s2, adding polyether and polyester into a reaction kettle, raising the temperature to 105 ℃, reducing the pressure to-0.095 MPa, dehydrating in vacuum for 30 minutes, removing the vacuum, reducing the temperature to 80 ℃, adding 1, 6-hexamethylene diisocyanate, stirring for 3 hours at the rotating speed of 400 rpm, adding neopentyl glycol 2, 2-dimethyl-3-hydroxypropionate and dioctyl phthalate, and stirring for 30 minutes at the rotating speed of 400 rpm to obtain a solution A;
s3, pumping the solution A into a synthesis kettle, keeping the pressure of the synthesis kettle at-0.1 MPa, sequentially adding 3-hydroxyethyl-1, 3-oxazolidine, cobalt naphthenate and a coupling agent at room temperature of 25 ℃, and stirring for 10 minutes at 450 revolutions per minute to obtain a solution B;
s4, adding kaolin and calcium carbonate into the solution B, keeping the pressure of the synthesis kettle at-0.1 MPa, stirring at the room temperature of 25 ℃ for 5 hours at 450 rpm, and discharging to obtain the waterproof environment-friendly coating.
The coupling agent is brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane, and the preparation process of the brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane is as follows: brominated bisphenol A epoxy resin and acetone are mixed according to the mass ratio of 1: 3 adding the mixture into a three-neck flask filled with nitrogen, stirring the mixture for 10 minutes at the rotating speed of 120 revolutions per minute, uniformly mixing the mixture, and then adding N- (2-N-benzyl aminoethyl) -3-aminopropyl trimethoxy silane which is 2 times of the weight of brominated bisphenol A epoxy resin, stirring the mixture at the rotating speed of 90 revolutions per minute at room temperature, and reacting the mixture for 60 minutes to obtain a reactant; and (3) distilling the reactant at 50 ℃ and the vacuum degree of-0.1 MPa under reduced pressure to remove acetone to obtain the brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane.
The flame retardant property test was performed on the waterproof environment-friendly coating prepared in example 5. Fire retardance: the test was carried out as specified in GB/T15442.4-1995, the flame resistance time: the test was carried out as specified in GB/T15442.2-1995. The results were: fire retardance: the mass loss is 1.9g, and the carbonization volume is 8cm3(ii) a The flame retardant time was 40 min. The waterproof environment-friendly coating prepared in example 5 is tested according to the building material industry standard JC/T894-2001 of the people's republic of China, and the test result is as follows: water impermeability (0.3MPa, 30 minutes): is impermeable to water; the wet base surface bond strength was 1.8 MPa.
Test example 1
The flame retardant property test was performed on the waterproof and environment-friendly coating prepared in examples 1 to 4. Fire retardance: the test was carried out as specified in GB/T15442.4-1995, the flame resistance time: the test was carried out as specified in GB/T15442.2-1995. Specific test data are shown in table 1.
Table 1: fire retardant and flame retardant time test data sheet
Test example 2
The waterproof and environment-friendly coatings prepared in examples 1 to 4 were tested according to the building material industry standard JC/T894-2001 of the people's republic of China. The test results are shown in Table 2.
Table 2: waterproof performance test result table
In the embodiment 2 of the invention, brominated bisphenol A epoxy resin is adopted to modify N- (2-N-benzyl aminoethyl) -3-aminopropyl trimethoxysilane, so that the flame retardance and the waterproof performance are greatly improved. The reason for this is probably that bromine is introduced into the coupling agent, so that the coupling agent has good flame retardant effect and the dispersibility of the system is improved.
Claims (6)
1. The preparation method of the waterproof environment-friendly coating is characterized by comprising the following steps:
s1, weighing the following raw materials in parts by weight: 25-30 parts of polyester, 48-52 parts of polyether, 1.5-4.5 parts of softener, 15-25 parts of kaolin, 5-15 parts of calcium carbonate, 0.3-0.7 part of coupling agent, 0.4-0.9 part of 3-hydroxyethyl-1, 3-oxazolidine, 0.3-0.6 part of catalyst and 15-20 parts of 1, 6-hexamethylene diisocyanate;
s2, adding polyether and polyester into a reaction kettle, raising the temperature to 110 ℃ for 100-;
s3, pumping the solution A into a synthesis kettle, keeping the pressure of the synthesis kettle between-0.12 and-0.08 MPa, and sequentially adding 3-hydroxyethyl-1, 3-oxazolidine, a catalyst and a coupling agent at the room temperature and stirring at 600 revolutions per minute for 5 to 15 minutes to obtain a solution B;
s4, adding kaolin and calcium carbonate into the solution B, keeping the pressure of the synthesis kettle between-0.12 MPa and-0.08 MPa, stirring at the room temperature for 2-4 hours at 600 rpm under the condition of 300-; the coupling agent is brominated bisphenol A epoxy resin modified N- (2-N-benzyl aminoethyl) -3-aminopropyltrimethoxysilane;
the preparation process of the brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane comprises the following steps: brominated bisphenol A epoxy resin and acetone are mixed according to the mass ratio of 1: (2-4) adding the mixture into a three-neck flask filled with nitrogen, stirring the mixture for 5 to 15 minutes at the rotating speed of 60 to 180 r/min, uniformly mixing the mixture, adding N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane, the weight of which is 1.5 to 2.5 times that of the brominated bisphenol A epoxy resin, into the mixture, and stirring the mixture at the rotating speed of 60 to 180 r/min at room temperature for reacting the mixture for 50 to 80 minutes to obtain a reactant; the reaction product is placed at the temperature of 45-55 ℃ and the vacuum degree of-0.12 to-0.09 MPa, and acetone is removed by reduced pressure distillation, so that brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane is obtained;
the softener consists of 30 wt% of dioctyl phthalate and 70 wt% of neopentyl glycol 2, 2-dimethyl-3-hydroxypropionate.
2. The preparation method of the waterproof environment-friendly coating according to claim 1, characterized in that: the catalyst is one or a mixture of cobalt naphthenate, dibutyltin dilaurate and stannous octoate.
3. The preparation method of the waterproof environment-friendly coating according to claim 1, characterized in that: the particle size of the kaolin is 1000-1500 meshes; the calcium carbonate is light calcium carbonate with the particle size of 1000-1500 meshes.
4. The preparation method of the waterproof environment-friendly coating according to claim 1, characterized in that: the polyester is unsaturated polyester resin, and the acid value is 10-30 mgKOH/g; the hydroxyl value of the polyether is 15-45 mgKOH/g; the epoxy equivalent of the brominated bisphenol A epoxy resin is 300-500g/eq, and the bromine content is 10-30 wt%.
5. The preparation method of the waterproof environment-friendly coating according to claim 1, characterized in that: the method comprises the following steps:
s1, weighing the following raw materials in parts by weight: 28 parts of polyester, 50 parts of polyether, 2.1 parts of 2, 2-dimethyl-3-hydroxypropionic acid neopentyl glycol ester, 0.9 part of dioctyl phthalate, 20 parts of kaolin, 10 parts of calcium carbonate, 0.5 part of coupling agent, 0.6 part of 3-hydroxyethyl-1, 3-oxazolidine, 0.5 part of cobalt naphthenate and 18 parts of 1, 6-hexamethylene diisocyanate;
s2, adding polyether and polyester into a reaction kettle, raising the temperature to 105 ℃, reducing the pressure to-0.095 MPa, dehydrating in vacuum for 30 minutes, removing the vacuum, reducing the temperature to 80 ℃, adding 1, 6-hexamethylene diisocyanate, stirring for 3 hours at the rotating speed of 400 rpm, adding neopentyl glycol 2, 2-dimethyl-3-hydroxypropionate and dioctyl phthalate, and stirring for 30 minutes at the rotating speed of 400 rpm to obtain a solution A;
s3, pumping the solution A into a synthesis kettle, keeping the pressure of the synthesis kettle at-0.1 MPa, sequentially adding 3-hydroxyethyl-1, 3-oxazolidine, cobalt naphthenate and a coupling agent at room temperature of 25 ℃, and stirring for 10 minutes at 450 revolutions per minute to obtain a solution B;
s4, adding kaolin and calcium carbonate into the solution B, keeping the pressure of the synthesis kettle at-0.1 MPa, stirring at the room temperature of 25 ℃ for 5 hours at 450 rpm, and discharging to obtain the waterproof environment-friendly coating;
the coupling agent is brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane, and the preparation process of the brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane is as follows: brominated bisphenol A epoxy resin and acetone are mixed according to the mass ratio of 1: 3 adding the mixture into a three-neck flask filled with nitrogen, stirring the mixture for 10 minutes at the rotating speed of 120 revolutions per minute, uniformly mixing the mixture, and then adding N- (2-N-benzyl aminoethyl) -3-aminopropyl trimethoxy silane which is 2 times of the weight of brominated bisphenol A epoxy resin, stirring the mixture at the rotating speed of 90 revolutions per minute at room temperature, and reacting the mixture for 60 minutes to obtain a reactant; and (3) distilling the reactant at 50 ℃ and the vacuum degree of-0.1 MPa under reduced pressure to remove acetone to obtain the brominated bisphenol A epoxy resin modified N- (2-N-benzylaminoethyl) -3-aminopropyltrimethoxysilane.
6. A waterproof environment-friendly coating prepared by the preparation method of any one of claims 1 to 5.
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| CN106047128A (en) * | 2016-01-22 | 2016-10-26 | 鞍山亿嘉达防水科技材料有限公司 | Single-component polyurethane polyureas waterproof paint and preparation method thereof |
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| CN106047128A (en) * | 2016-01-22 | 2016-10-26 | 鞍山亿嘉达防水科技材料有限公司 | Single-component polyurethane polyureas waterproof paint and preparation method thereof |
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